STRUCTURAL AND SOLID-STATE P-31 NMR-STUDIES ON A NOVEL FLUOROTRIS(TRIPHENYL-PHOSPHINE)COPPER(I) ADDUCT

被引:12
作者
HEALY, PC
HANNA, JV
KILDEA, JD
SKELTON, BW
WHITE, AH
机构
[1] GRIFFITH UNIV,BRISBANE NMR CTR,NATHAN,QLD 4111,AUSTRALIA
[2] UNIV WESTERN AUSTRALIA,DEPT PHYS & INORGAN CHEM,NEDLANDS,WA 6009,AUSTRALIA
关键词
D O I
10.1071/CH9910427
中图分类号
O6 [化学];
学科分类号
0703 ;
摘要
The synthesis of the title compound as its triphenylphosphine/methanol solvate, [(PPh3)3CuF].4PPh3.4MeOH, is reported together with characterization by solid-state P-31 CP-MAS n.m.r. and single-crystal X-ray diffraction. Crystals are trigonal, space group P3, with a 14.453(5), c 15.388(6) angstrom. The structure refined to a final R value of 0.049 for 1926 'observed' [I > 3-sigma-(I)] reflections. The (PPh3)3CuF molecule lies on a crystallographic threefold axis. Cu-F is 2.115(9) angstrom, and Cu-P 2.323(3) angstrom. The solid-state P-31 n.m.r. spectrum is dominated by peaks from each of the four solvated PPh3 molecules at -1.6, -5.4, -10.6 and -14.2 ppm with respect to 85% H3PO4. The quartet of lines arising from the ligands coordinated to the copper atom shows an average chemical shift of -5 ppm and approximately equal line spacings of 1.0 kHz.
引用
收藏
页码:427 / 432
页数:6
相关论文
共 9 条
  • [1] LEWIS-BASE ADDUCTS OF GROUP-11 METAL(I) COMPOUNDS .28. SOLID-STATE P-31 CROSS-POLARIZATION MAGIC-ANGLE SPINNING NUCLEAR-MAGNETIC-RESONANCE AND STRUCTURAL STUDIES ON THE MONONUCLEAR 3-1 ADDUCTS OF TRIPHENYLPHOSPHINE WITH COPPER(I) HALIDES
    BARRON, PF
    DYASON, JC
    HEALY, PC
    ENGELHARDT, LM
    PAKAWATCHAI, C
    PATRICK, VA
    WHITE, AH
    [J]. JOURNAL OF THE CHEMICAL SOCIETY-DALTON TRANSACTIONS, 1987, (05): : 1099 - 1106
  • [2] CRYSTAL + MOLECULAR STRUCTURE OF TRIPHENYL-PHOSPHORUS
    DALY, JJ
    [J]. JOURNAL OF THE CHEMICAL SOCIETY, 1964, (OCT): : 3799 - &
  • [3] TRIPHENYLPHOSPHINE OXIDE AS A CRYSTALLIZATION AID
    ETTER, MC
    BAURES, PW
    [J]. JOURNAL OF THE AMERICAN CHEMICAL SOCIETY, 1988, 110 (02) : 639 - 640
  • [4] COORDINATION STABILIZED COPPER(I) FLUORIDE - CRYSTAL AND MOLECULAR-STRUCTURE OF FLUOROTRIS(TRIPHENYLPHOSPHINE)COPPER(I).ETHANOL (1-2), CU(PPH3)3F.2ETOH
    GULLIVER, DJ
    LEVASON, W
    WEBSTER, M
    [J]. INORGANICA CHIMICA ACTA-ARTICLES, 1981, 52 (02): : 153 - 159
  • [5] Ibers J. A., 1974, INT TABLES XRAY CRYS, VIV
  • [6] P-31 NMR-STUDIES OF SEVERAL PHOSPHINES IN THE SOLID-STATE
    PENNER, GH
    WASYLISHEN, RE
    [J]. CANADIAN JOURNAL OF CHEMISTRY-REVUE CANADIENNE DE CHIMIE, 1989, 67 (11): : 1909 - 1913
  • [7] SOBOLEV AN, 1983, ZH STRUKT KHIM, V24, P123
  • [8] STEWART JM, 1983, TR901 U MAR COMP SCI
  • [9] Verkade J. G., 1987, PHOSPHORUS 31 NMR SP